定制各类格氏试剂

问题:请问如何合成这个物质?
类型:求助 (悬赏分:3分)
提问:qqqqa
等级:
版块:有机化学问题(jimuwei,fpcwin1211,netpanda,yjgzfl,Ftian,)
信誉:56%
回复:5
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时间:2006-09-20 12:38:33  编辑    加入/取消收藏    订制/取消短消息    举报该贴    

23847-08-7
CA INDEX NAME:
2H-Azepin-2-one, 1,1'-dithiobis[hexahydro-
FORMULA:
C12H20N2O2S2
N,N'-Dilactam disulfide
回复人:tangyyer,★★★★★ (有空来逛逛my blog: http://tangyyer.blog.hexun.com) 时间:2006-10-06 10:12:14   编辑 1楼
看看DE3012895:The reaction of lactams with S2Cl2 to give the disulfides I (n = 1-5) was carried out in DMF in the presence of NaO2CH or NaOAc. Thus, 113 g e-caprolactam was homogenized with 270 kg DMF and 90 kg NaO2CH and treated with 67.5 g S2Cl2 to give 85% I (n = 3);
US3525737:I and II are prepd. by treating lactams with SCl2 and S2Cl2, resp. Thus, 8.5 g 2-pyrrolidinone in 50 ml trichloroethylene and 8.7 g pyridine is treated dropwise with 5 g SCl2 to give 60% I (n = 2), m. 134-6? Also prepd. was I (n = 4), m. 134-7? The following II were prepd. (n and m.p. given): 2, 97-101? 3, 67-73? 4, 128-34? 6, 81-3


回复人:guozengfa, (真诚,喜欢交朋友) 时间:2006-10-06 11:19:41   编辑 2楼
hehe,我看不懂


回复人:hyw30,▲▲ (学无止尽 奋斗不息) 时间:2006-10-08 16:02:14   编辑 3楼
可否分三步合成:
第一步酰胺的闭环生成内酰胺,然后氮的卤代,再与二硫化钾反应.


回复人:qqqqa, (a) 时间:2006-10-20 17:43:01   编辑 4楼
如何卤代,不知氯气可否?


回复人:Ace, (我为合成疯狂!) 时间:2006-10-21 10:41:46   编辑 5楼
用氯气可能有杂质产生,还是用S2CL2比较好




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